Determination of fluoride and chloride in nickel ore by ion chromatography
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Abstract:
The simultaneous determination of fluoride and chloride contents in nickel ore by ion chromatography was established.The sample was decomposed by H2SO4.After water steam distillation at 160-180℃,the fluoride and chloride in testing solution would be released and absorbed by NaOH solution,realizing the separation from matrix and other elements.Then,the contents of fluoride and chloride were determined by ion chromatography.The high-capacity IonPacAS23 anion separation column(4 mm×250 mm) and IonPacAG23 protection column(4 mm×50 mm) were used as chromatographic column and 20 mmol/L NaOH solution was used as eluent.Fluoride and chloride were detected with conductivity detector.The results showed that the peak area of fluoride and chloride had good linear relationship with their contents in the range of 1-25 μg/mL.The correlation coefficients(R) were 1.000 0 and 0.999 6 for fluoride and chloride respectively.The determination results of fluoride and chloride in sample showed high precision.The recoveries of standard addition were all greater than 95%.Keywords:
Ion chromatography
Thermal conductivity detector
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A method for determination of fluoride content in zinc concentrates was established.By alkali fusion together with semi-melting method,the influence of a large number of sulfur on sample pretreatment was removed.The floride that to be analyzed was separated from many other heavy metal ions in ores using water vapor distillation.After alkali fusion and water vapor distillation process,the interference in ion chromatographic determination was eliminated to the greatest extent and the detection limit was decreased.Sodium carbonate(2.5mmol/L)and sodium bicarbonate(3.5mmol/L)mixture solution was used as eluent and SH-AC-1(200mm×4.6mm ID)was used as anion analytical column for separation.A suppressed conductivity detector was for detection.As a result,the linear ranges of the method for fluoride in the zinc concentrate were 0.004% ~0.5% and the correlation coefficient was0.999 6.The standard addition recoveries were 97%~102%and the relative standard deviation was less than 4.0%.The sample detection limit was 0.0004%.The method effectively expands the contents of fluoride in zinc concentrate that can be determined.
Sodium carbonate
Ion chromatography
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A simple and rapid method for the determination of fluoride in the range above 10ppm up to 48.67 wt.% for CaF2 within a total time of 15 minutes is described. Samples are mixed with PbO2 in the ratio 1 : 3; and the fluoride is liberated in an induction furnace within ca. 10 minutes. The fluoride is collected in a 0.025 molar sodium-hydroxide solution and after adding 100ml buffer (1M sodium citrate, 1M sodium chloride), the solution is filled up to 250ml with distilled water, and measured by an ion-selective electrode using the technique of standard addition. Analyses of five international reference samples show excellent accuracy from 0.5 to 3% with a standard deviation of less than 4% (e.g., for a fluoride contents of 442ppm in Andesite AGV-1).
Fluorine
Distilled water
Sodium hydroxide
Sodium fluoride
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Hydrochloric acid
Anhydrous
Sodium hydroxide
Cryolite
Sodium fluoride
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Abstract Lanthanum hydroxide supported on alumina has been studied to sorb fluoride ion from aqueous solutions. The adsorbent is effective in decreasing fluoride ion concentration from 7 mM to 0.003 mM in the pH range 5.7–8.0. The rate constant for sorption was found to be 6x10‐2 min‐1. The sorption of fluoride is Langmuir type and its capacity is 0.82 m M F‐/g of the adsorbent. The sorption selectivity shows that fluoride removal is affected by the presence of phosphate and sulphate but not affected by chloride, bromide iodide and nitrate ions. Alumina impregnated with lanthanum hydroxide has adsorption capacity in the range 0.340–0.365 mM/g. The removal of fluoride from industrial waste water is more than 96%. Fluoride ion sorbed can be eluted from the adsorbent with 10 mL of 0.1 M NaOH and the column can be reused after being conditioned with 10 mL of 1 mM hydrochloric acid. Results obtained by batch as well column methods are in good agreement with each other.
Hydrochloric acid
Lanthanum
Langmuir adsorption model
Activated alumina
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Citations (30)
A study to find a better mobile phase for use in the rapid determination of inorganic anions such as fluoride, chloride, nitrite, phosphate, nitrate and sulfate ions by indirect photometric ion chromatography is presented. The eluent optimized was a weak-alkaline (pH 7.3) buffer solution containing 0.7 mM potassium hydrogenphthalate-0.1 mM sodium tetraborate-0.5 mM boric acid-0.1 mM HEPPS-0.05 mM sodium hydrogencarbonate-5 % butanol. The problem of the system peak otherwise encountered was eliminated by judicious choice of the alkalinity of the buffer solution. The eluent did not show any pH drift typically caused by dissolution of carbon dioxide, and was able to separate the phosphate ion completely from the chloride. Whole anions above described were determined within 15 min.
Ion chromatography
Alkalinity
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Studied on the influence of chloride ion to nitrate determination when using ion chromatography to analyze low amount of nitrate in the hydrochloric acid solution.By adding the silver oxide,the chloride ion was removed and the pH of hydrochloric acid solution was adjusted to be neutral.Then the sample was injected in to the ion chromatography to determine the concentration of nitrate.The RSD of this method is 0.05%~1.5%(n3),and the average yield is 99.3%.
Hydrochloric acid
Silver nitrate
Ion chromatography
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The deleterious effects on the quality of soil and ground waters of electrolytes discharged as a result of salts used by the tanning industry is of concern now more than ever. The electrolyte is usually in the form of chloride and sulphate and thus it is necessary to determination chloride ion and sulphate ion in tanning effluents. The determination of chloride ion and sulphate ion in leather pickling liquor is important to determine the salt's contribution to the total salt concentration of the sewage for each process. The aim of this work is to apply LPIC (without using a suppressor column) to the quantitative determination of chloride ion and sulphate ion in pickle liquor. Tests of precision, recovery and linear range were also conducted to evaluate the above method. The results show that the coefficients of variation are less than 4.77% or 3.76% with recoveries of 99.95% and 102.31% for chloride ion and sulphate ion respectively. Two calibration curves were obtained over the concentration range of 10 to 30 mg/L for chloride and 30 to 300 mg/L for sulphate. The detection limits of the method developed for chloride ion and sulphate ion are 0.144 and 2.853 mg/L respectively. LPIC performed without a suppressor column is shown to be suitable as a method for quantitative determination of chloride ion and sulphate ion in leather pickling liquor.
Pickling
Ion chromatography
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Through the determination of chloride and sulfate,the contents of salt and sodium sulfate in natural trona ore can be obtained.At present analysis methods are inefficient,causing disadvantages,such as having a time-consuming process,easy pollution and low production efficiency.This study establishes the analysis method which detects chloride and sulfate in natural trona ore by the ion chromatography-suppression conductivity measurement.The anions were dissolved into the solution by hot water and the chloride and sulfate were separated by using AG-19 type anion protect column and AS-19 type anion separation column with 30 mmol/L KOH as the eluent.The interference from carbonate ion was eliminated by a Carbonate Removal Device(CRD).Under optimal conditions,the detection limits of chloride and sulfate were 0.01 and 0.02 mg/L,respectively.The recoveries were between 100.9%-104.1% and the precisions of the method(RSD,n=10) were less than 2.5%.The results for the actual samples were consistent with those obtained by the titration method.This method is simple and avoids interferences by the complicated components of the sample and the buffer solution system,while also being economical,accurate,giving good reproducibility and high sensitivity.
Ion chromatography
Sodium carbonate
Sodium sulfate
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Sodium carbonate
Electroanalytical method
Ion selective electrode
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Microamounts of chloride ion in high-purity sodium hydroxide was determined directly by the chloride turbidimetric method.The optimal analysis conditions were that the determination wavelength was 440nm and the liner range was 0～8ug/mL.The absolute difference of parallel determination was less than 0.0005%,which met national standards.The recovery of chloride ion in different levels was measured in high-purity sodium hydroxide,and the result was 96.5%～102.9%.The experimental method was accurate and simple,and it could be applied in routing inspection.
Sodium hydroxide
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